Ammonia saturator and tar removal apparatus



July 21, 1953 c. OTTO 2,646,345

AMMONIA SATURATOR AND TAR REMOVAL APPARATUS Filed Feb. 2, 1950 INVENTOR 4o CHRL OTTO ATTORNEY Patented July 21, 1953 as lo to ApplicatlonFebruary 2, 1950, Serial o."141',963 a The general object of the present invention is to provide a spray saturator for use in converting I the ammonia content of a gas having a small ammonia content, such as coke oven gas, into ammonium sulphate in a scrubbing chamber into which finely divided acidified ammonium sulphate liquor is sprayed into a stream of gas under a pressure substantially highen-forexample ten pounds per square inch higher, thanthe pressure of the external atmosphere. v I

I have heretofore invented anddeveloped-spray saturators for operation with a: gas" pressure difieringlittle from the pressure of the -atmos--, phere, such as the saturators disclosed in mycopending application, Serial No. 14,902, filed March 15, 1948,v and in earlier applications of which said application, Serial No.,l4,902,. is a continuation-in-part.-

A practically important object of the present invention is to'adapt a spraysaturator of the general type disclosed insaid co-pending application for use in recovering ammonia from gas under pressure appreciably above that of the atmosphere, without requiring materialchanges in the general structure of the s'atiirator. In the preferred form of the present invention, the liquor space is located in the-lower portion-ofa verticallyelongated tank, with the; spray scrubbing space directly above thebath-space, and

advantageously having a conica1 pervious baflie wall extending across the tank between the :upper end of the scrubbing space and-a gasoutlet.

Aspecificv object of .theinvention is to provide a'bath liquor overflow and liquor return arrangement, including relatively simple and effective provisions forseparating tar from the overflowdisposed, tank, I, having: an'upper end-portion 2 shown, as of largercrosssection than thesubjacent bodyportion of the' tank-.; The lower end portion 3; of the tank serves as adesupersaturating and crystallizer bath space. which includes the hopper bottom portion 4- of the tank fanda short lower section ,of the cylindrical-tank space below an unobstructed scrubbing space 5 which constitutes the bulk of; the tank space. The gas to be scrubbed-passes under pressure "into 'the' lower portion of -the. scrubbing space 5 through an inlet opening 6 to which gas is supplied-by an external gas supply pipe shown as including a pipe el'bow 1 immediately adjacent "the inlet I5. The gas passes away from the saturator through an outlet 81 adjacent its upper endandopening into a gas I ofi take pipe 9. An acid catcher ID in the form of a pervious barrier or bafile wall of conical form, is interposed between the-gasoutlet 8 and the scrubbing space 5 below the acid catcher. The gas scrubbing provisions comprise an upper spray nozzle l I; a plurality of intermediate spray nozzles l2, and a lower spray nozzle I3. Each of the nozzles H, 12 and I3 may Well'be of the commercially available anti-clogging, atomizing type disclosed in the Eneas Patent No. 1191264,

ing liquor andfor returningto the bath the liquor fromrwhich the tar has -been separatedwithout significant reduction in the pressure of'the liquor. .The various features of novelty which characterize my invention 'arapointed out with particularity in the claims annexed to and forming a part of thisspecification. Fora better under standing'of the invention, however; its advantages, and specific objects attained withits use, reference should "be had to the accompanying drawingand descriptive matterin whichI have illustrated and described preferred embodiment of'the invention 1 I "5 Theone figureof the accompanying drawing is a diagrammatic representation of a spray saturator and associated recirculating and tar removingprovisio'ns. I Y ;;n g

In the drawing, I have illustrated an embodiment- =of the invention -comprising'- a vertically of June 23, 1914. a I

Advantageously thei conical acid catcher wall l0 has aconicalangle'of 10 or more, and has a peripheral edge extending into engagement with the tank shell, andis suitably supported by the latter; The pervious wall Ill may be formed of saddle bricksor Rauschi-g rings, or by some other pervious bafiie wall arrangement. The pervious wall In needs to be cleaned from time to time, and this may be effected by spraying hot water through nozzles I4 carried by supply pipes, which extends down into the tank through its upper end wall, and are distributed and arranged to dis charge water against substantially all portions of the upper surface of the wall ID. A substantial portion of the liquor thus sprayed on to the pervious conical wall ID will drain to the peripheral edge of the wall In and then fiowin film form downward along the inner surface of the tank wall, carrying with it the dissolved salt which may have previously accumulated on and in the wall 'I 0 and on the tank-wall.

' The scrubbing liquor sprayed into the gas moving upward through the scrubbing space 5 comprises a dilute solution of ammonium sulphate preferably saturated and admixed with from five to ten per cent by weight of sulphuric acid which has been'withdrawn from. the bath space 3 and entraining (ammonium sulphate crystals. The

downward through the top wall of the tank and through the central portion of the acid catcher wall Hi to supply liquor to the nozzle ll ,;-car'ried at the lower end of said branch. Other discharge:

branches l8 of the pipe l6, extend through the tank wall and supply liquor to spray nozzles l2;

All or one or more of the loranch pipes I1 and 18 may include a throttling valve IQ for use in regulating the relative amounts of liquor discharged through the different nozzles. The spray nozzle l3= receives liquor through the branch 22' from the outlet pipe 22 of a pump 23. The pump 23 has its inlet pipe 23' arranged to withdraw satu-' rated liquor and entrained crystals from the lower end of the hopper bottom portion 4 of the tank. The pipe 22' includes a portion. 22 for passing crystals and the liquor entraining them I to separating apparatus of any usual or suitable form. Such apparatus as is explained in said application, Serial No. 14,902 ordinarily includes a centrifugal or other drier for separating crystalsufrom entraihing liquor and" drying them, and a pipe such as the pipe 24'for returning liquor to-the-erystallizr bath'space.

Liquor overflows from the bath space through a U-shaped p'ipe 25"havin'g one uprisinglegextending through the tank wall and having its upper end open at the desired bath top level. The other leg of the pipe 25 terminates in a gooseneck section 26,- which extendsthrough the wall of a small vertically disposed, closed'tar pot or decanter 2.1. As' shown, the pipe section 25 extending into the decanter tank 21 has its discharges through its dowri'turhed end into a vertically-disposed sleeve 28'. The latter has its openupper end above, and its open lower end substantially below the decanter liquor level. That level is fixed by an overflow connection 29, shown as comprising a horizontal portion extend ing through the decanter shell with an uprising portion open at its upper end in the decanter; The other end of the pipe 2-9 opens into a tax tank 30 above the tar level 3|, normally maintained in the latter.

In the operation contemplated. tar is discharged from the tank 30' through a discharge pipe 32 duringintermittent periods in which ,a discharge valve 33 in thepipe 32 is open. There is a continuousgravitational flow of liquor out of the lower hopper bottom end of the decanter 21' through an outlet pipe 34. The latter includes an uprising discharge end portion 35 which opens into the upper portionof a closed liquor reservoir and return tank 36; The liquor flow into the tank 36 through the pipe 34-, is normally of relatively small volume and may be regulated or controlled by the movement toward and away from its open upper endofa manually adjustable valve or throttling member 31. As shown, the latter is carried at the lower end of a stem 39'. which extends vertically through the upper end wall of the tank 36 and is provided at its outer upper end with a handle 40 for moving the mem= ber 31 toward and away from the discharge end 35' of the pipe 34. Liquorcollectingin the lowerend of the return tank 36, may be returned to the bath space 3 continuously or intermittently by means of a pump 40. As shown, the latter has a valved inlet pipe 4| connected to the lower end of the hopper bottom portion of the tank 36. The pump 40 discharges tangentially into the bath space 3 through the pump outlet pipe 42. The latter extends through the bottom wall 4 of the tank; l", "ahd"h'as" its open end 42' discharging tangentially into the peripheral portion of the bath space, near the upper end of the latter.

' In accordance with the present invention, the upper end of each of the tanks 21, 30 and 3B is connected to a pressure equalizing pipe 43 through an individual uprising connection includinga valve 44 and opening through the top wall of the tank. The pipe 43 is connected through a pipe 45 including a valve 46 to the gas outlet pipe 9, so that when the valves 44 and 46 are open, the gas pressure in the upper ends of theXtan-ks 21; 30 and 36 is substantially equal to the pressure of the gas moving through the tank I.- With the pressures in the upper ends of the tanks- 21,. 39 and 36-, thus equalized with the gas pressure in-, the saturator outlet pipe 9, the liquor level in the decanter tank 21 will be maintained approximately constant at an overflowlevei fixed by the pipe 29- and which may be, but little below the liquor level in the bath space 3. The liquor level in the tank 30 may fluctuate betweena maximum but" little below the liquor level irrithetank I, and a lower level which has no relation to the levels in any of the other tanksand depends simply on the adjustment of the discharge valve 33 through which the tar is discharged inte a 'tar well or receirit'acle not shown iiithe drawing;

It is possible to automatically control the tar ieveiin the tank it b the use of means adjusting the valv'e'r'esponse to changes in the height or liquid level in that term. in practice, howeveiyme dischargeval v'e 33 may well be menu-- as controlled and opened at intermittent in te'rvalsorhythrettlingthe valve as required to keep" the tarlevel in the tank 30 suitably below the reverie the tank 21-. When the discharge valve 33 is'closed the tar level in the tank- 30 gradually builds up as tar overflows from the decanter tank 2-1-5 The previously mentioned liquor return pipe 24 may-be directly connected to the tank I at a level below, but adjacent the upper end of the crystallizer sr'i'ace 3. As shown; however; the pipe 24 is connected to the space 3 throu h the oiitlet pipe 42 of: the pump-40. The liquor may be moved from the separatorinto the pipe 24' by a pump in some cases. in other cases, the separator may well be located at a level suffi= iently high above" the bath space to drain by gravity into said space directly, or through the pipe" 24. 1

Whilei'fi' accordahcevv'ith the provisions of the statutea l have illustrated and described the best form of embodiment of my inventiorinow known to the, it-will be apparent to those skilled in the a-rt that changesmay he made in the form of the apparatus disclosed without departing from the spirit oi my invention as set forth in the appended claims; and that in some casescer-' tain features of my inventions may be used to advantage without a corresponding useof other features. 7

. 'ii-avine now described my invention, what I claim as new and desire to secure by Letters Patent, ist

1. In spray saturator and tar eliminating apparatus for the production of ammonium sulphate from distillation gas having a small ammonia content and comprising a vertically disposed tank structure enclosing a chamber including an upper. substantially unobstructed gas scrubbing space and a liquor desupersaturating and crystallizing bath space below said scrubbing space and arranged to receive liquor, tar and crystals from the latter, an overflow conduit connected to said structure and having its inlet end open to said chamber at a level-intermediate the upper and lower ends of said chamber andv operative to discharge bath liquorand tar at said level, said structure having a'gas inlet and a gas outlet respectively opening to lower and open to said tar tank at a third level below said second level, a second closed tar tank into which said second overflow conduit discharges at a fourth level below said second level and below the top of said second tar tank, a gas pressure equalizing connection between said gas scrubbing space and the upper end portion of each of said =tar tanks, said second tar tank having a tar outlet opening to the tank at a level below said second level, and means for regulating flow through the last mentioned outlet.

2. The improvementspecified in claim 1, comprising means including a return pump for withdrawing liquor. from the lower portion of said 3. The improvement as specified in claim 2, in

'7 which the means for returning liquor and enunper portions of said scrubbing space spray V nozzles mounted in said structure to discharge into said scrubbing space, pumping and conduit means connected to said structure to withdraw liquor and crystals'from said bath space, and to pass liquor and crystals through said spray nozzles'into said scrubbing space through said spray nozzles and having an outlet for passing liquor and crystals to crystalseparating apparatus, and means for adding make-up acid to the liquor passed into said'scrubbing space, the improvement comprising conduit means for connecting said gas inlet to a source of distillation gas under pressure to maintain a gas pressure in said trainedlcrystals from the first tar tank to the saturator tank includes a closed reservoir, a conduit opening from the first tar tank adjacent its lower end anddischarging into said reservoir at a level below the first mentioned level, said reservoir having an outlet below the first men-' -tioned level and connected to the inlet of said return pump and means for equalizing the gas pressure in the upper end of said reservoir with the gas pressure in said scrubbing space.

CARL o'rTo.

scrubbing space substantially above the pressure of the atmosphere, a first closed tar tank connected to said overflow conduit to receive liquor and tar overflowing from'said bath space, said overflow conduit having its outlet end opening into said tar tank'at a second level below the first mentioned level and below the top of said tar tank, the latter having an; overflow outlet References Cited in the file of this patent 'UNITED STATES PATENTS first tar tank and returning it to said bath space." 

1. IN SPRAY SATURATOR AND TAR ELIMINATING APPARATUS FOR THE PRODUCTION OF AMMONIUM SULPHATE FROM DISTILLATION GAS HAVING A SMALL AMMONIA CONTENT AND COMPRISING A VERTICALLY DISPOSED TANK STRUCTURE ENCLOSING A CHAMBER INCLUDING AN UPPER SUBSTANTIALLY UNOBSTRUCTED GAS SCRUBBING SPACE AND A LIQUOR DESUPERSATURATING AND CRYSTALLIZING BATH SPACE BELOW SAID SCRUBBING SPACE AND ARRANGED TO RECEIVE LIQUOR, TAR AND CRYSTALS FROM THE LATTER, AN OVERFLOW CONDUIT CONNECTED TO SAID STRUCTURE AND HAVING ITS INLET END OPEN TO SAID CHAMBER AT A LEVEL INTERMEDIATE THE UPPER AND LOWER ENDS OF SAID CHAMBER AND OPERATIVE TO DISCHARGE BATH LIQUOR AND TAR AT SAID LEVEL, SAID STRUCTURE HAVING A GAS INLET AND A GAS OUTLET RESECTIVELY OPENING TO LOWER AND UPPER PORTIONS OF SAID SCRUBBING SPACE, SPRAY NOZZLES MOUNTED IN SAID STRUCTURE TO DISCHARGE INTO SAID SCRUBBING SPACE, PUMPING AND CONDUIT MEANS CONNECTED TO SAID STRUCTURE TO WITHDRAW LIQUOR AND CRYSTALS FROM SAID BATH SPACE, AND TO PASS LIQUOR AND CRYSTALS THROUGH SAID SPRAY NOZZLES INTO SAID SCRUBBING SPACE THROUGH SAID SPRAY NOZZLES AND HAVING AN OUTLET FOR PASSING LIQUOR AND CRYSTALS TO CRYSTAL SEPARATING APPARATUS, AND MEANS FOR ADDING MAKE-UP ACID TO THE LIQUOR PASSED INTO SID SCRUBBING SPACE, THE IMPROVEMENT COMPRISING CONDUIT MEANS FOR CONNECTING SAID GAS INLET TO A SOURCE OF DISTILLATION GAS UNDER PRESSURE TO MAINTAIN A GAS PRESSURE IN SAID SCRUBBING SPACE SUBSANTIALLY ABOE THE PRESSURE OF THE ATMOSPHERE, A FIRST CLOSED TAR TANK CONNECTED TO SAID OVERFLOW FROM CONDUIT TO RECEIVE LIQUOR AND TAR OVERFLOWING FROM SAID BATH SPACE, SAID OVERFLOW KCONDUIT HAVING ITS OUTLET END OPENING INTO SAID TAR TANK AT A SECOND LEDVEL BELOW THE FIRST EMENTIONED LEVEL AND BELOW THE TOP OF SAID TAR TANK, THE LATTER AND BELOW THE TOP OF SAID OPEN TO SAID TAR TANK AT A THIRD LEVEL BELOW SAID SECOND LEVEL, A SECOND CLOSED TAR TANK INTO WHICH SAID SECOND OVERFLOW SAID SECOND LEVEL AND BELOW FOURTH LEVEL BELOW SAID SECOND LEVELS AND BELOW THE TOP OF SAID SECOND TAR TANK, A GAS PRESSURE EQUALIZING CONNECTION BETWEEN AND GAS SCRUBBING SPACE AN THE UPPER END PORTION OF EACH OF SAID TAR TANKS, SAID SECOND TAR TANK HAVING A TAR OUTLET OPENING TO THE TANK AT A LEVEL BELOW SAID SECOND LEVEL, AND MEANS FOR REGULATING FLOW THROUGH THE LAST MENIONED OUTLET. 